Fractional distillation apparatus



April 23, 1946. w, s'gov ETAL Y 2,398,807

- ERACTIONAL DISTILLATION APPARATUS Filed Dec. 51, '1942 ELIE-=7 INVENTORS WAR NER-E .SCOVILLond THOMAS J.WAL5H ATTORNEYS PatentedApr. 23, 1946 FRACTIONAL DISTILLATION APPARATUS Warner E. Scovill, Cleveland Heights, and Thomas J. Walsh, Cleveland, Ohio, assignors to The Standard Oil Company, Cleveland, Ohio, a corporation of Ohio Application December 31, 1942, Serial No. 470,718-

9 Claims. (01. 202- 161) This invention relates to distillation; and it is among the objects of the invention to provide accuracy in distillation control, and particularly for precision operation, as in laboratory columns and industrial fractionating apparatus of larger scale where unusual exactness of control is desired.

To the accomplishment of the foregoing and related ends, the invention, then, comprises the features hereinafter fully described, and particu-' larly pointed out in the claims, the following description and the annexed drawing setting forth in detail certain illustrative embodiments of the invention, these being indicative however, of but a few of the various ways in which the principle of the invention may be employed In said annexed drawing:

Fig. l is a vertical sectional view, partly broken,

showing distillation apparatus embodying the invention; Fig. 2 is a similar view showing a modification; and Figs. 3-7 inclusive are similarly fragmentary side ,elevational views showing further modifications of certain details.

Referring more particularly to Fig. 1, there is shown a fractionating column having a distilling portion or chamber} and a condensing portion or chamber 3 which provides condensate liquid or reflux for the fractionating portion below. The distilling or iractionating portion provides suitable contact between up-rising vapors and downwardly-travelling reflux in the general manner of fractional distillation, and such surfaces may, depending upon the size of'the particular appa-' ratus and preferences in detail, involve more or less elaborate filling, which may take the form of suitable horizontal plates or plural vertical surfaces or packed filling units, asdesired. The con= densing chamber or section, arranged to deliver reflux, may for instance involve a condensing surface 5 on the exterior of which liquid forms and runs down to its lower extremity. The condenser includes suitable baffling, as 6, whereby cooling fluid, water or other in accordance with the particular material being distilled, may be supplied by inlet connection l and be discharged by outlet connection 8. Outlet connection it permits discharge of uncondensed vapors or gases. A supply inlet connection l2 at the lower portion of the distilling chamber permits introduction of the material to be distilled, and this may be introduced at suitable vapor-disengaging temperature or may be heated by suitable means, detail of which is immaterial for the present purposes. Advantageously, the connection 62 may have suitable valved branches by which the one opening in the distillation chamber may also serve for withdrawal of un-vaporized residuum.

A collector is is arranged to catch liquid proceeding from the condenser, anddirect it into a calibrated chamber is. The collector may be small and allows vapors to pass by freely, and e. g. it may be of suitable funnel-like character with discharge into the calibrated chamber in convenient assembly, and. the latter is provided with valve means by which it may be controlled as desired, to collect the reflux liquid and determine its rate of production. The chamber i5 is accordingly calibrated in units comparable with the size of the fractionating column, fdr instance cubic centimeters for small laboratory apparatus, and larger units for larger apparatus, etc. The valve means as shown in Fig. l is a movable valve member it, guided on a guide support I? which is suitably secured to the distllling chamber so as to allow movement of the valve member up and down in closing or opening with respect, to the valve seat iii, the closing movements being occasioned by passing current through an electromagnetic coil is (suitably sealed against permeation of distillation material) actuating an iron armature 20 in the valve member. The magnet i9 is suitably controlled by an electric circuit Cwith switch S and source of current supply. Opening or downward movement of the valve member is occasioned by gravity on cessation of the flow of the electric current.

In operation, the vapors rising from the lower portion of the distilling chamber 2 proceed upwardly through the fractionating section, and vapors still uncondensed encounter the cooled condenser surface 5 and the condensed liquid, falls from the lower end of the condenser to a distributor 2| which may be of any desired detail to supply the liquid across the distilling section. Reflux liquid reaching the collector it goes into the calibrated chamber l5, and with the valve it open may proceed on through, in regular course. When it is desired to determine the rate of reflux flow, the electromagnetic coil i9 is energized on closing the circuit by the switch means, and the armature 20 being drawn upward by the magnet closes the valve 86. With walls of glass. as in small apparatus, or glass sights in larger apparatus, the filling may be timed, and the rate thus ascertained. Generally, in distillation procedure it is not desired to interrupt the normal flow of reflux'for other thanshort test periods, and desirably the size of the calibrated chamber, It may be correlated to the size of the fractionating column, such that for example a fifteen secmination.

Instead of positioning the calibrated chamber below the iractionating fllling, in. some cases it is desired to determine the rate of reflux liquid flow to the top of the distilling chamber, and the calibrated chamber may be located between the condenser and the distilling chamber as shown at la, in Fig. 2. The detail of the valve mechanism in such position may be as afore-described. Or, as a further modification the valve member IGa may be on a valve lever 23 pivoted at 24, and having at its further end an armature 20a to be attracted and drawn upwardly (to close the valve) by an electromagnet Illa. With such construction, the valve llia is normally open and allows liquid to flow on through. -When it is desired to.

determine the flow rate, the switch is closed and the magnet I911 is energized, and the armature a being drawn upwardly'closes the valve member Ilia. The rate being timed, as above-described, the circuit is opened, andthe armature 20a drops down onto its normal lug-support 25, thereby opening the valve lGa.

In Fig. 3, instead of having a valve member on a lever, it may more simply be a ball-valve lib, to be drawn from its valve seat l8b by energizing the magnet 19b. The timing and determining of the reflux rate is accomplished as already described, the electric circuit to magnet 19b being tie-energized to allow the valve member IN: to roll down and close the valve for the requisite time for collecting and determining the reflux,

. 0nd period may be sufliclent for a test detering out through the side of the column may also be incorporated. when the valve member is down in closed position, such connection is closed, and it is opened when the valve member is raised. With valve members having tapered valving projections, a variable outlet opening is had, which results in flotation of the buoyant valve member at a different level for difierent amounts of reflux.

In some cases, instead of having magnetically controlled valve operation with an electric circuit allowing control from as remote a point as desired, it may be preferred to operate the valve 'manually, in which case a valve I61, Fig. 7, is

positioned in the outlet conduit 3| from the calibrated chamber IS in an accessible position just outside the lateral wall of the column.

It will be understood that the various detail constructions of the valve may be incorporated in the outlet of the calibrated chamber as in Figs. 1 and 2. And in general, in operation, the liquid coming from above flows into the calibrated chamber and normally passes on through the open outlet below, but when it is desired to deterand then by energizing the magnet IS!) the valve is opened to allow normal flow on through. The valve member I6!) is formed of magnetic material or may have magnetic material on its interior. Instead of a single magnet for controlling the ball valve, one magnet I90, Fig. 4, may be arranged to open the valve by drawing the ball valve member 16c oil? from the valve sea We to come to rest in a depression 21 provided for that purpose in the floor of the calibrated chamber l5c. A transitory energizing oi the magnet I90 thus serves to open the valve and it remains open on de-energizing the circuit. To close the valve, the magnet He is energized, and -the transitory action thereof serves to draw the ball valve away from its-retaining position 21, whereupon it rolls down into closing position onthe valve seat lllc. Instead of the valve member being of ball type, it may be in the form as shown in Fig. 5, in which the valve member 16d has a tapering projection 21 through the outlet opening of the calibrated chamber, the valve member closing on the valve seat lBd when in lower position, and having lugs 28 to maintain it generally in centered position. With the valve member formed of magnetic metal or having magnetic metal within, control is effected by magnet IN, the valve being opened when the electric circuit is energized, and closed by gravity when the cirvalve member centered in its various positions.- Operation is again provided by the magnet Me which attracts magnetic metal of which the valve is formed or which is enclosed within the valve member. An ofi-take liquid connection as leadmine the reflux flow rate, the valve is closed and the rise of liquid in the calibrated chamber is timed, whereupon the valve is again opened for accustomed operation. The distillation may correspondingly be controlled as to its detail, rate of application of heat to the material to be distilled, rate of separation, etc., as desired.

Other modes of applying the principle of the invention may be employed, change being made as regards the details described, provided the features stated in any of the following claims, or the equivalent of such, be employed.

We therefore particularly point out and distinctly claim as our invention:

1. Fractional distillation apparatus, comprising a single vertical tubular column havinga distilling chamber and enclosing fractionating surfaces, at least a part of said column being transparent, a condensing chamber within said column in direct vertical alignment for receiving vapors from said fractionating surfaces, a calibrated chamber inside said column directly below said condensing chamber for receiving liquid therefrom and passing the same on below, the calibrations being visible from outside said column through said'transparent portion, and a valve to control the outlet of the calibrated chamber.

2. Fractional distillation apparatus as described in claim 1 wherein the valve is a ball valve member within the calibrated chamber and movable to and from its outlet opening, a recess at one side of said opening and wherein the apparatus includes in the bottom of the calibrated chamber wherein the ball valve member may rest, magnetic metal in' said ball valve member, a magnet to draw said ball valve member from the opening of the calibrated chamber to position in said recess, and electric circuit means for controlling said magnet.

3. Fractional distillation apparatus as described in claim 1 wherein the valve is a valve member reciprocable to control the outlet of the calibrated chamber and having a tapered projection in said opening and being of slight buoyancy to float on a small amount of reflux liquid and wherein the apparatus includes, magnetic material in said valve member, a magnet to attract such magnetic material and control the valve member, and an electric circuit to control the magnet.

4. Fractional distillation apparatus comprising a single vertical tubular column having a distilling chamber and enclosing fractionating surfaces,

a for actuating said valve.

5. Fractional distillation apparatus, comprising a single vertical tubular column having a distilling chamber and enclosing fractionating surfaces, a condensing chamber within said column in direct vertical alignment for receiving vapors from said fractionating surfaces, a calibrated chamber inside said column directly below said condensing chamber for receiving liquid from said condensing chamber and passing the same on below, a valve member inside said column to control the outlet of the calibrated chamber, and electric circuit means allowing remote control of said valve member, at least a portion of said column being transparent adjacent said calibrated chamber, whereby the calibrations of said chamber are visible from outside said column.

6. Fractional distillation apparatus, comprising a single vertical tubular colunm having a distilling chamber and enclosing fractionating surfaces, at least a part of a wall of said column being constructed of transparent material, a condensing chamber within said column in direct vertical alignment for receiving vapors from said fractionating surfaces, a calibrated chamber inside said column directly below said condensing chamber andvisible through said transparent material for receiving liquid from said condensing chamber and passing the same on below, a valve reciprocable to control the outlet of the calibrated chamber, a magnet toactuate said valve, and an electric current to control said magnet.

7. Fractional distillation apparatus, comprising a single vertical tubular column having a dis-' tilling chamber and enclosing fractionating surfaces, at least a part of a wall of said column being transparent, a condensing chamber within said column in direct vertical alignment for re ceiving vapors from said fractionating surfaces, a calibrated chamber inside said column directly below said condensing chamber and visible through the transparent part of the wall of said column for receiving liquid from said condensing chamber and passing the same on below, a valve to control the outlet of said calibrated chamber, a guide on which said valve is slidably mounted, magnetic metal in said valve, a magnet to attract such magnetic metal and actuate said valve, and an electric circuit for controlling the magnet.

8. Fractional distillation apparatus, comprising a single vertical tubular column having a dis.

tilling chamber and enclosing fractionating surfaces, at leastv a part of a wall of said column being transparent, a. condensing chamber within said column in direct vertical alignment for receiving vapors from said fractionating surfaces,

a calibrated chamber inside said column directly below said condensing chamber and visible through the transparent part of the wall of said column for receiving liquid from said condensing chamber and passing same on below, a valve for closing the outlet of the calibrated chamber, magnetic metal in said valve, a magnet to attract such magnetic metal and actuate said valve against the action of gravity, and an electric circuit for energizing said magnet. 1

9. Fractional distillation apparatus, comprising a single vertical tubular column having a distilling chamber and enclosing fractionating surfaces, at least a part of a wall of said column being transparent, a condensing chamber within said column in direct vertical alignment for -receiving vapors from said fractionating surfaces, a calibrated chamber inside said column directly below said condensing chamber and visible through the transparent part of the wall of said column for receiving liquid from said condensing chamber and passing same on below, a ball valve member to control the'outlet of the calibrated chamber, magnetic metal in said ball valve member, a magnet to attract such magnetic metal and control said ball valve member, and an electric circuit to control the magnet.

WARNER E. SCOVILL. THOMAS J. WALSH. 

